This dataset contains dissolved organic matter (DOM) characteristics from surface water samples collected at 100 urban stream locations in the greater Boston, Massachusetts metropolitan area. Samples were collected four times (September 2021, November 2021, April 2022, and July 2022) to capture spatial and seasonal variation in DOM characteristics. Fluorescent optical properties were measured on filtered water samples to understand the chemical composition of DOM. Excitation-Emission Matrices (EEMs) were measured using a Horiba Aqualog spectrometer. DOM characteristics were quantified using both standard fluorescence and absorbance metrics as well as through parallel factor (PARAFAC) analysis.